CN105254609B - The extracting method of blueberry anthocyanin - Google Patents
The extracting method of blueberry anthocyanin Download PDFInfo
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- CN105254609B CN105254609B CN201510847783.1A CN201510847783A CN105254609B CN 105254609 B CN105254609 B CN 105254609B CN 201510847783 A CN201510847783 A CN 201510847783A CN 105254609 B CN105254609 B CN 105254609B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- Coloring Foods And Improving Nutritive Qualities (AREA)
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Abstract
The present invention provides the extracting method of blueberry anthocyanin.Extracting method is as follows：First, in flash extracter, by blueberry and the broken extraction of extract solution, extract solution is filtered to obtain；2nd, by extract solution and oil phase hybrid extraction, oil phase and aqueous phase are separated to obtain；3rd, oil phase is mixed into back extraction with citric acid extraction liquid, obtains aqueous phase extracted；4th, after mixing aqueous phase and aqueous phase extracted, anthocyanidin filtrate is separated to obtain using membrane separation process, then anthocyanidin filtrate is concentrated, acquisition anthocyanidin is dried.Blueberry is efficiently effectively crushed in a short time using flash extracter, while under high velocity agitation, the contact and collision of increase extract solution and broken blueberry material reduce extraction time.The strip stage of the aqueous citric acid solution of step 3 is provided with simultaneously, and using anthocyanidin property more stable in citric acid solution, the anthocyanidin in oil phase is stripped to aqueous citric acid solution.Therefore, the impurity content in anthocyanidin extract solution is few, and the purity of the anthocyanidin obtained through UF membrane is high.
Description
Technical field
The present invention relates to the extracting method in anthocyanidin extractive technique field, more particularly to blueberry anthocyanin.
Background technology
Anthocyanidin (anthocyanins) is also known as anthocyanidin, is the water-soluble natural color that a class is widely present in plant
Element, belongs to flavone compound, exists more in the form of glucosides, also referred to as anthocyanin.Anthocyanidin is used as a kind of natural food colour, peace
Entirely, nontoxic, aboundresources, and with certain nutrition and pharmacological action, have huge in terms of food, cosmetic, medicine
Application potential, blueberry anthocyanin makes it well received in health food, medical industry unique health-care effect of human body eyesight.Flower
Blue or green element has very strong oxidation resistance, can eliminate human free radical, protect the health cell, activates senile cell, improves human body
Vigor, cancer-resisting effect is the senior fruit of health generally acknowledged in the world substantially.
Therefore, how to extract anthocyanidin from plant turns into the emphasis studied at present.At present, mostly from early stage extraction with after
Continuous two aspects of separating-purifying are studied respectively.Mainly have adsorption-desorption method, membrane separation process in terms of separating-purifying, enzyme process and
High performance liquid chromatography.Wherein generally use adsorption-desorption method, this method, which needs to use substantial amounts of solvent, to be carried out desorption and wash
It is de-, a large amount of solvents are wasted, the wasting of resources is caused.And membrane separation process have carry out at normal temperatures, separation process does not have phase-state change,
There is no chemical change, good, the strong adaptability of selectivity, low power consumption and other advantages are gradually widely used in the later separation of anthocyanidin
Purification.But membrane separation process mainly isolates object by the setting of molecular cut off, is obtained by extraction due to early stage
In extract solution in addition to anthocyanidin, also containing other materials, such as colloid, starch, carbohydrate, fat, organic acids and base organic
Material, therefore, causes that the impurity content in the anthocyanidin that is obtained using membrane separation process is high, purity is low.
The content of the invention
For the drawbacks described above and problem of prior art, it is an object of the invention to provide the extracting method of blueberry anthocyanin.
During solving the separating-purifying in existing anthocyanidin extraction process, because the impurity component contained in the extract solution of early stage is more,
The technical problem for causing the purity of the anthocyanidin of extraction low when subsequently using membrane separation process.
In order to achieve the above object, the present invention provides following technical scheme：
The extracting method of blueberry anthocyanin, through the following steps that realize：
Step 1: blueberry and extract solution are put into the extraction vessel of flash extracter, flash extracter is opened, is broken
It is broken to extract, obtain broken extract solution；Broken extract solution is filtered into obtain extract solution and filter residue；
Step 2: adding grease type oil phase into the extract solution of step one, stir and evenly mix, obtain the milkiness that oil phase is continuous phase
Liquid, stands, and layering separates to obtain oil phase and aqueous phase；The volume ratio of the extract solution and grease type oil phase is 1 ﹕ 1~2；
Step 3: adding extract in the oil phase obtained into step 2, stir, then stand, be layered, separating to extract
Aqueous phase and raffinate oil phase；Wherein, the extract use mass concentration for 0.2%~0.5% aqueous citric acid solution, oil phase and
The volume ratio of extract is 1 ﹕ 3~5；
Step 4: the aqueous phase extracted of the aqueous phase of step 2 and step 3 is mixed, anthocyanidin extract solution is obtained；Anthocyanidin is carried
Take liquid to separate to obtain anthocyanidin filtrate using membrane separation process, then anthocyanidin filtrate is concentrated, acquisition anthocyanidin is dried.
Further, in step one, the extract solution is to include the ethanol and 0.2%~0.5% that mass concentration is 60%
Citric acid mixed solution；The concrete operations of the broken extraction are：Extract solution temperature is risen to 80 DEG C~90 DEG C of temperature
Under, flash extracter is opened, 1~2min of broken extraction is carried out, is then quenched to less than 60 DEG C, continuation is broken to extract 10min.
Further, in step one, it is 2~5L of 500g ﹕ to control blueberry quality and the ratio of extracting liquid volume.
Further, in step 2, the grease type oil phase is edible oil esters, or for available for medicine or cosmetic
Grease class in product.
Further, in step 2, the grease type oil phase includes but is not limited to following several：Sesame oil, soybean oil, certain herbaceous plants with big flowers
Flower seed oil, peanut oil, walnut oil, safflower seed oil, corn oil, olive oil, camellia seed oil, natural VE, pungent certain herbaceous plants with big flowers acid glycerol
Ester, isopropyl palmitate, oleic acid or isopropyl myristate.
Further, in step 4, filtered in the membrane separation process using microfiltration membranes, milipore filter and/or NF membrane
Separation.
Further, in step 4, used in the membrane separation process and retain relative molecular weight for 200,000 organic film.
Further, in step 4, anthocyanidin filtrate is concentrated, dry concrete operations are：Anthocyanidin filtrate is added
In downward film evaporator, concentrated under vacuum, discharge ethanol, obtain concentrate；Then using lyophilized technique to concentration
Processing is dried in liquid, obtains anthocyanidin.
Blueberry is efficiently effectively crushed in a short time using flash extracter in the step one of the present invention, simultaneously
Under high velocity agitation, the contact and collision of increase extract solution and broken blueberry material, reduces extraction time, improves extraction efficiency.It is excellent
Selection of land, carries out broken extraction, overcomes what should not be heated in existing extraction process in short time at a high temperature of 80 DEG C~90 DEG C
Technical problem, further increases extraction efficiency, and recovery rate is up to 4%.
In the extract solution extracted through step one in addition to anthocyanidin, also containing other materials, such as colloid, starch, sugar
Class, fat, organic acids and base etc., are mostly organic species, according to similar compatibility principle, in step 2, utilize grease type oil
Above-mentioned impurity (non-purpose extract) in extract solution is extracted in oil phase.In the step 2, because anthocyanidin is phenol
Class material, has small part anthocyanidin and is extracted into oil phase unavoidably, therefore, and the citric acid water of step 3 is provided with the present invention
The strip stage of solution, using anthocyanidin property more stable in citric acid solution, by the anthocyanidin in oil phase be stripped to
Aqueous citric acid solution.Therefore, the impurity content in the anthocyanidin extract solution of step 4 is few, follow-up to use what is extracted during membrane separation process
The purity of anthocyanidin is high, and wherein Cyanidin and Chinese herbaceous peony cellulose content reaches 80%.
Embodiment
Below in conjunction with embodiments of the invention, technical scheme is clearly and completely described, it is clear that
Described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the implementation in the present invention
Example, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made is belonged to
The scope of protection of the invention.
Embodiment 1
The extracting method of blueberry anthocyanin, through the following steps that realize：
Step 1: 1kg blueberries and 10L extract solutions are put into the extraction vessel of flash extracter, by extract solution temperature liter
At a temperature of 90 DEG C, flash extracter is opened, broken extraction 2min is carried out, is then quenched to less than 60 DEG C, continue broken carries
10min is taken, broken extract solution is obtained；Broken extract solution is filtered into obtain extract solution and filter residue；The extract solution is to include mass concentration
The mixed solution of ethanol and 0.2% citric acid for 60%.
Step 2: adding isopropyl palmitate oil phase into the extract solution of step one, stir and evenly mix, it is scattered to obtain extract solution
Phase, oil phase are the emulsion of continuous phase, are stood, and layering separates to obtain oil phase and aqueous phase；The body of the extract solution and grease type oil phase
Product is than being 1 ﹕ 2；It is different that the organic impurity such as colloid, starch, carbohydrate, fat, organic acids and base in extract solution are extracted into palmitic acid
In propyl ester oil phase, wherein, the anthocyanidin of fraction can be also extracted into isopropyl palmitate oil phase.
Step 3: adding extract in the oil phase obtained into step 2, stir, then stand, be layered, separating to extract
Aqueous phase and raffinate oil phase；Wherein, the extract uses mass concentration for 0.2% aqueous citric acid solution, oil phase and extract
Volume ratio be 1 ﹕ 5；
Step 4: the aqueous phase extracted of the aqueous phase of step 2 and step 3 is mixed, anthocyanidin extract solution is obtained；Anthocyanidin is carried
Take liquid to use retention relative molecular weight to carry out membrane separation process for 200,000 organic film and separate to obtain anthocyanidin filtrate, then anthocyanidin is filtered
Liquid is added in downward film evaporator, is concentrated under vacuum, is discharged ethanol, is obtained concentrate；Then lyophilized technique is used
Processing is dried to concentrate, 30g anthocyanidin is obtained.
The recovery rate of the extracting method of the blueberry anthocyanin of the present embodiment 1 is 3%, extracts corn flower in obtained anthocyanidin
Element and Chinese herbaceous peony cellulose content 80%.
Embodiment 2
The extracting method of blueberry anthocyanin, through the following steps that realize：
Step 1: 1kg blueberries and 6L extract solutions are put into the extraction vessel of flash extracter, extract solution temperature is risen to
At a temperature of 80 DEG C, flash extracter is opened, broken extraction 2min is carried out, is then quenched to less than 60 DEG C, continue broken extract
10min, obtains broken extract solution；Broken extract solution is filtered into obtain extract solution and filter residue；The extract solution is to include mass concentration to be
The mixed solution of 60% ethanol and 0.5% citric acid.
Step 2: adding isopropyl palmitate oil phase into the extract solution of step one, stir and evenly mix, it is scattered to obtain extract solution
Phase, oil phase are the emulsion of continuous phase, are stood, and layering separates to obtain oil phase and aqueous phase；The body of the extract solution and grease type oil phase
Product is than being 1 ﹕ 2；It is different that the organic impurity such as colloid, starch, carbohydrate, fat, organic acids and base in extract solution are extracted into palmitic acid
In propyl ester oil phase, wherein, the anthocyanidin of fraction can be also extracted into isopropyl palmitate oil phase.
Step 3: adding extract in the oil phase obtained into step 2, stir, then stand, be layered, separating to extract
Aqueous phase and raffinate oil phase；Wherein, the extract uses mass concentration for 0.5% aqueous citric acid solution, oil phase and extract
Volume ratio be 1 ﹕ 3；
Step 4: the aqueous phase extracted of the aqueous phase of step 2 and step 3 is mixed, anthocyanidin extract solution is obtained；Anthocyanidin is carried
Take liquid to use retention relative molecular weight to carry out membrane separation process for 200,000 organic film and separate to obtain anthocyanidin filtrate, then anthocyanidin is filtered
Liquid is added in downward film evaporator, is concentrated under vacuum, is discharged ethanol, is obtained concentrate；Then lyophilized technique is used
Processing is dried to concentrate, 40g anthocyanidin is obtained.
The recovery rate of the extracting method of the blueberry anthocyanin of the present embodiment 2 is 4%, extracts corn flower in obtained anthocyanidin
Element and Chinese herbaceous peony cellulose content 85%.
The assay method of anthocyanidin content is as follows in the present invention：
Liquid phase testing conditions are：C18 chromatographic columns (4.6mm × 250mm × 5 μm, purchased from Akzo Nobel N.V. of Sweden,
Kromasil C18 chromatographic columns), mobile phase is the glacial acetic acid solution of methanol -0.2% (80: 20, v/v), and flow velocity is 1.0mL/min,
Column temperature is 25 DEG C, ultraviolet detection wavelength 530nm, each μ L of sample introduction 10.Standard items are Cyanidin -3-O- glucosides, 3- Portugals
Polyglycoside peonidin.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be contained
Cover within protection scope of the present invention.Therefore, protection scope of the present invention described should be defined by scope of the claims.
Claims (5)
1. the extracting method of blueberry anthocyanin, it is characterised in that through the following steps that realize：
Step 1: blueberry and extract solution are put into the extraction vessel of flash extracter, flash extracter is opened, broken carry is carried out
Take, obtain broken extract solution；Broken extract solution is filtered into obtain extract solution and filter residue；The extract solution is that to include mass concentration be 60%
Ethanol and 0.2%~0.5% citric acid mixed solution；The concrete operations of the broken extraction are：By extract solution temperature
Rise at a temperature of 80 DEG C~90 DEG C, open flash extracter, carry out 1~2min of broken extraction, be then quenched to less than 60 DEG C,
Continue broken extraction 10min；It is 2~5L of 500g ﹕ to control blueberry quality and the ratio of extracting liquid volume；
Step 2: adding grease type oil phase into the extract solution of step one, stir and evenly mix, obtain the emulsion that oil phase is continuous phase,
Stand, layering separates to obtain oil phase and aqueous phase；The volume ratio of the extract solution and grease type oil phase is 1 ﹕ 1~2；
Step 3: adding extract in the oil phase obtained into step 2, stir, then stand, be layered, separate to obtain aqueous phase extracted
With raffinate oil phase；Wherein, the extract uses mass concentration for 0.2%~0.5% aqueous citric acid solution, oil phase and extraction
The volume ratio of liquid is 1 ﹕ 3~5；
Step 4: the aqueous phase extracted of the aqueous phase of step 2 and step 3 is mixed, anthocyanidin extract solution is obtained；By anthocyanidin extract solution
Anthocyanidin filtrate is separated to obtain using membrane separation process, then anthocyanidin filtrate is concentrated, acquisition anthocyanidin is dried；Wherein, by anthocyanidin
Filtrate concentration, the concrete operations dried are：Anthocyanidin filtrate is added in downward film evaporator, carried out under vacuum dense
Contracting, discharges ethanol, obtains concentrate；Then processing is dried to concentrate using lyophilized technique, obtains anthocyanidin.
2. the extracting method of blueberry anthocyanin according to claim 1, it is characterised in that in step 2, the grease type
Oil phase is edible oil esters, or for available for the grease class in medicine or cosmetics.
3. the extracting method of blueberry anthocyanin according to claim 2, it is characterised in that in step 2, the grease type
Oil phase includes but is not limited to following several：Sesame oil, soybean oil, sunflower oil, peanut oil, walnut oil, safflower seed oil, corn
Oil, olive oil, camellia seed oil, natural VE, pungent certain herbaceous plants with big flowers acid glyceride, isopropyl palmitate, oleic acid or myristic acid isopropyl
Ester.
4. the extracting method of blueberry anthocyanin according to claim 1, it is characterised in that in step 4, the UF membrane
It is separated by filtration in method using microfiltration membranes, milipore filter and/or NF membrane.
5. the extracting method of blueberry anthocyanin according to claim 4, it is characterised in that in step 4, the UF membrane
Used in method and retain relative molecular weight for 200,000 organic film.
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| CN105686069B (en) * | 2016-03-25 | 2017-05-31 | 广东省金叶科技开发有限公司 | A kind of tobacco extract and preparation method thereof and its purposes |
| CN106701482A (en) * | 2016-12-30 | 2017-05-24 | 山东景芝酒业股份有限公司 | Rapid preparation method of healthcare mulberry wine |
| CN107760057A (en) * | 2017-10-30 | 2018-03-06 | 潍坊友容实业有限公司 | A kind of Suaeda salsa Betacyanins extracting method |
| CN114223837A (en) * | 2021-12-23 | 2022-03-25 | 江西丹霞生物科技股份有限公司 | Preparation process of oil-soluble anthocyanin |
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| CN103509834B (en) * | 2013-10-16 | 2015-07-08 | 合肥工业大学 | Method for preparing high bio-availability blueberry anthocyanin |
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